▎ 摘　　要

NOVELTY - Preparation of three-dimensional composite hydrogen evolution electrode involves adding graphene oxide to deionized water, adding nickel sulfamate, nickel chloride and ammonium chloride, obtaining a composite plating solution, fixing a processed nickel substrate on inner wall of a cylindrical reactor as a cathode, and pure nickel tube at central axis of the cylindrical reactor as an anode, circulating a corrosion preventive pump for the composite plating solution between the reactor and an external reservoir, subjecting to electrodeposition, washing with deionized water, and drying. USE - Preparation of three-dimensional composite hydrogen evolution electrode (claimed). ADVANTAGE - The method enables preparation of three-dimensional composite hydrogen evolution electrode having high specific surface area, uniform and stable coating structure, and excellent hydrogen evolution performance. When current density is 100 mA/cm2, the overpotential of hydrogen evolution reaction using the electrode is reduced from 240 mV to 190 mV. DETAILED DESCRIPTION - Preparation of three-dimensional composite hydrogen evolution electrode involves pre-treating a nickel substrate before electrodeposition, providing the substrate in a container filled with deionized water, ultrasonically processing for 5 minutes, processing with 3 M hydrochloric acid solution for 30 seconds, washing with deionized water, drying, preparing graphene oxide by Hummers method, adding 0.1-5 g graphene oxide to 1 L deionized water, ultrasonically processing at 100-300 W for 1-6 hours, obtaining an uniform, brown graphene oxide dispersion, adding 350 g nickel sulfamate, 10 g nickel chloride and 30 g ammonium chloride to 1 L graphene oxide dispersion, ultrasonically processing at 100-300 W for 1-6 hours, obtaining a composite plating solution having pH of 3.5-3.8, fixing the processed substrate on inner wall of a cylindrical reactor as an electrodeposition cathode, and pure nickel tube at central axis of the cylindrical reactor as an electrodeposition anode, circulating a corrosion preventive pump for the composite plating solution between the cylindrical reactor and an external reservoir, subjecting to electrodeposition at 45 degrees C and 3 A/dm2 for 10-100 minutes, washing resultant composite coating with deionized water, and drying.